Abstract : Although alkyd resins have been the object of considerable research during the past 20 years, a general method for the analysis of polyols has not appeared in the literature. The type and amount of polyol used in the production of alkyd resins greatly influences the physical and chemical properties of alkyd-based coatings; therefore, it is important that quality control, relative to polyol content, be exercised. This report describes a procedure which can be used for the identification of a broad spectrum of polyhydric alcohols. In addition, polyols can be determined quantitatively. Sample manipulation is minimal and a simultaneous determination is made with resins containing more than one polyol. A resin sample is dried and then refluxed with butylamine. Polyols released during the aminolysis are reacted with a trimethylsilyl reagent forming their corresponding trimethylsilyl ethers. Separation of the polyol derivatives is performed on a 16 foot silicone grease column. (Author)